CN104411637B - Method for producing gamma-2CaO. SiO2 - Google Patents

Method for producing gamma-2CaO. SiO2 Download PDF

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Publication number
CN104411637B
CN104411637B CN201380034489.8A CN201380034489A CN104411637B CN 104411637 B CN104411637 B CN 104411637B CN 201380034489 A CN201380034489 A CN 201380034489A CN 104411637 B CN104411637 B CN 104411637B
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mass
2caosio
manufacture method
raw mixture
sio
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CN104411637A (en
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庄司慎
盛冈实
樋口隆行
山本贤司
吉野亮悦
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Denka Co Ltd
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Denki Kagaku Kogyo KK
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/24—Alkaline-earth metal silicates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/18—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mixtures of the silica-lime type
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/345—Hydraulic cements not provided for in one of the groups C04B7/02 - C04B7/34
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/345—Hydraulic cements not provided for in one of the groups C04B7/02 - C04B7/34
    • C04B7/3453—Belite cements, e.g. self-disintegrating cements based on dicalciumsilicate
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

Provided is a method for producing gamma-2Cao. SiO2, which has a high carbonation rate, has a high degree of whiteness, does not comprise any toxic substances, does not inhibit the setting or hardening of cement, has a reduced energy cost during calcination, and has a high yield. The raw mixture is a combination of the raw materials of slaked lime, which is produced as a by-product after producing acetylene by reacting calcium carbide and water, and of silica. In addition, the raw mixture is adjusted so that CaO/SiO2 has a molar ratio of 1.6-2.0 inclusive and a total alkali content of 0.05-1.00 mass%, or so that CaO/SiO2 has a molar ratio greater than 2.0 but not exceeding 2.4, and a total alkali content not exceeding 0.50 mass%. Said raw mixture is calcinated in a rotary kiln at a calcination temperature of 1300-1600oC to produce gamma-2Cao. SiO2.

Description

γ-2CaO·SiO2Manufacture method
Technical field
The invention mainly relates to γ-the 2CaOSiO that can be utilized as cement material2Manufacture method.
Background technology
2CaO·SiO2It is known to have α types, β types, γ types etc..Wherein, stable at normal temperatures is β types and γ types.Known β types One of composition as portland cement (portland cement), with the hydraulicity although the hydraulicity is weak.The opposing party Face, although γ types do not have the hydraulicity, carbonating activity is high, and discovered in recent years is used as the useful of cement additive Property.Thus, 2CaOSiO2β types and γ types had been found that the purposes of the respective feature of performance, if therefore control can be established 2CaO·SiO2Crystal habit method, then it is industrially beneficial.
In pure 2CaO-SiO2System in, the 2CaOSiO of β types will not be generated2, and γ types can be formed as.As To 2CaOSiO2The factor that impacts of crystal habit, it is known to (1) ternary impact, the shadow of (2) cooling condition Sound, (3) oxidation-reduction atmosphere etc..
As ternary impact, it is known that if boron, phosphorus, barium, strontium, ferrum, aluminum, molybdenum for being contaminated with more than a certain amount of etc., β -2CaOSiO can be generated2(non-patent literature 1, non-patent literature 2, non-patent literature 3).
γ-2CaO·SiO2(patent documentation 1) is used as the admixture of the neutralization for suppressing cement concrete, additionally, Can also be by obtaining high perdurable concrete (patent text with forcing carbonized maintaining (carbonation curing) to be applied in combination Offer 2).
Prior art literature
Non-patent literature
Non-patent literature 1：Schwiete et al.,Zem.-Kalk-Gips,Vol.21,No.9,359,1968
Non-patent literature 2：Bavin Tian Chunfu (bavin field Pure husbands) etc., ceramic industry association will (Kiln industry Association meeting Chi), Vol.92, No.2, 71,1984
Non-patent literature 3：Niesel et al.Tonind-Ztg., Vol.93, No.6,197,1969
Patent documentation
Patent documentation 1：Japanese table patent WO2003/016234 public again
Patent documentation 2：Japanese Unexamined Patent Publication 2006-348465 publications
The content of the invention
Problems to be solved by the invention
The present invention provide whiteness it is high, without harmful substance, also the condensation of cement will not be hindered to harden, burning can also be cut down Into when the also high γ -2CaOSiO of cost of energy, yield2Manufacture method.
For solution to problem
The present inventor etc. has been repeated various researchs, as a result finds, the ripe stone of by-product after acetylene is produced by Acetylenogen. In grey raw material and siliceous raw material, although micro but comprising alkali composition, according to CaO/SiO2The scope of mol ratio is further in raw material Total alkali content in adding alkali composition in mixture to adjust raw mixture, thus generates γ -2CaOSiO2.Also, it was found that γ-the 2CaOSiO obtained by the method2Carbonating activity it is high, whiteness is high, without harmful substance, also without prejudice to cement Condensation hardening, be useful.
As described above, the present inventor etc. has carried out unremitting effort, with regard to γ -2CaOSiO2Manufacture method, find carbon Souring activity is high, whiteness is high, without harmful substance, also the condensation hardening of without prejudice to cement, can also cut down energy when burning till The also high γ -2CaOSiO of cost, yield2Manufacture method, so as to complete the present invention.
The present invention has following main idea.
1. a kind of γ -2CaOSiO2Manufacture method, it is characterised in that in rotary kiln with firing temperature 1300～ 1600 DEG C are burnt till raw mixture, and the raw mixture is compounded with making Acetylenogen. react with water to produce the ripe of by-product after acetylene Calx raw material and siliceous raw material, and carried out adjusting and making CaO/SiO2Mol ratio is more than 1.6 and less than 2.0, total alkali Measure as 0.05 mass %～1.00 mass %, or make CaO/SiO2Mol ratio is 0.50 more than 2.0 and for less than 2.4, total alkali content Below quality %.
2. γ -2CaOSiO according to above-mentioned 12Manufacture method, wherein, the brick of the clinkering zone of rotary kiln is magnesium Oxygen spinels or high-purity alpha-alumina class.
3. γ -2CaOSiO according to above-mentioned 1 or 22Manufacture method, wherein, hydrated lime feed contains 71～74 The CaO of quality %, the loss on ignition (LOI) of 23～25 mass %, the SiO of 0.5～1.5 mass %2, 0.2～0.35 mass % Fe2O3, 0.3～0.7 mass % Al2O3, MgO less than 0.2 mass %, any one be respectively less than the Na of 0.1 mass %2O、K2O、 And 1.0～1.5 mass % SO3。
4. γ -2CaOSiO according to any one of above-mentioned 1～32Manufacture method, wherein, siliceous raw material is silicon The dust (dust) of stone micropowder, silicon ash (silica fume), kieselguhr or vitreous silica.
5. γ -2CaOSiO according to any one of above-mentioned 1～42Manufacture method, wherein, hydrated lime feed And/or siliceous raw material has granularity of 90 mass % above by 150 μm of sieves.
6. γ -2CaOSiO according to any one of above-mentioned 1～52Manufacture method, wherein, to raw mixture Pelletize is carried out, the granules for obtaining are fed to rotary kiln.
7. γ -2CaOSiO according to above-mentioned 62Manufacture method, wherein, using pressing the matter of water/raw mixture Amount carries out pelletize than the water for being calculated as 10～30%.
8. γ -2CaOSiO according to any one of above-mentioned 1～72Manufacture method, wherein, in raw mixture Alkaloid substance be potassium carbonate and/or sodium carbonate.
9. γ -2CaOSiO according to any one of above-mentioned 1～82Manufacture method, wherein, firing temperature is 1450 DEG C～1550 DEG C.
The effect of invention
γ -2CaOSiO of the invention2Manufacture method, the γ -2CaOSiO for obtaining2Play carbonating activity Cost of energy, the yield that high, whiteness is high, will not also hinder condensing for cement to harden, can also cut down when burning till is also high equivalent Really.
Specific embodiment
Hereinafter, the present invention is described in detail.
It should be noted that the part, % in the present invention represents quality criteria in the case of without special provision.
γ -2CaOSiO described in the present invention2Refer to：With CaO and SiO2For the silicic acid in the compound of main component Dicalcium 2CaOSiO2One kind.Dicalcium silicate 2CaOSiO2There is α types, α ' types (α prime type), β types, γ types.This The bright dicalcium silicate for being related to γ types.
In the present invention, using hydrated lime feed (the calcium hydroxide original for making Acetylenogen. that by-product after generation acetylene is reacted with water Material).If using the raw material, the 2CaOSiO of γ types is obtained2.Even if using reagent calcium hydroxide, other can be used as industry Raw material and the Calx that obtains, also cannot the present invention γ -2CaOSiO2。
The composition that Acetylenogen. reacts the Calx of by-product after generation acetylene with water is set to carry out adding by the Calx to by-product Oxide benchmark meter after heat treatment, comprising 71～74% or so CaO, 23～25% or so loss on ignition (LOI), 0.5～ 1.5% or so SiO2, 0.2～0.35% or so Fe2O3, 0.3～0.7% or so Al2O3, MgO less than 0.2%, appoint One is respectively less than 0.1% Na2O、K2O, 1.0～1.5% or so SO3。
In the present invention, except the hydrated lime feed using by-product after making Acetylenogen. and water reaction generation acetylene, (CaO is former Material) outside, also using siliceous raw material (SiO2Raw material).
To siliceous raw material (SiO2Raw material) it is not particularly limited, it is possible to use Silicon stone micropowder, silicon ash, kieselguhr, tekite Dust of English etc..In order to obtain γ -2CaOSiO2, the also favourable one side of the presence of impurity.
Wherein, in the present invention, even if using highly purified siliceous raw material (SiO2Raw material), by using making Acetylenogen. and water Reaction produces the hydrated lime feed of by-product after acetylene, and γ -2CaOSiO are also obtained2。
In the present invention, total alkali content means Na contained in raw mixture2O、K2O、Li2The content (quality %) of O.
Alkaloid substance is not particularly limited, it is possible to use potassium carbonate, sodium carbonate etc..
Heat treatment method is not particularly limited.Can be burnt using rotary kiln, electric furnace, continuous tunnel furnace, shaft kiln, fluidized bed type Burn stove etc..Wherein, from from the viewpoint of continuous operation, cost performance, need to select rotary kiln.
Firing temperature is 1300 DEG C～1600 DEG C, is preferably 1400 DEG C～1550 DEG C, is more preferably 1450～1550 DEG C.It is low When 1300 DEG C, sometimes deterioration of efficiency, become raw burn, during more than 1600 DEG C, melt, not only operation becomes difficult, and Become easily to adhere to skinning (coating), sometimes yield is reduced.Herein described firing temperature refers to maximum temperature, rotary kiln In the case of, refer to the temperature of clinkering zone.
In present invention, it is desirable to by the CaO/SiO of raw mixture2Mol ratio is adjusted to 1.6～2.4.It is adjusted to more than 1.6 And when less than 2.0, need for total alkali content to be set to more than 0.05% and less than 1.00%, it is preferably set to more than 0.10% and 0.95% Below.In addition, by the CaO/SiO of raw mixture2Mol ratio be adjusted to more than 2.0 and for less than 2.4 when, need total alkali content Less than 0.50% is set to, less than 0.40% is preferably set to, or 0%.
The CaO/SiO of raw mixture2When mol ratio is less than 1.6, wollastonite, the silicoglaserite of by-product α types, γ -2CaO SiO2Containing ratio step-down.The CaO/SiO of raw mixture2When mol ratio is more than 2.4, by-product 3CaOSiO2, free lime, γ-2CaO·SiO2Containing ratio still step-down.
The granularity of hydrated lime feed and siliceous raw material is preferably regulated as making 150 μm of percent of pass be more than 90%, more preferably adjusts It is whole for make 100 μm of percent of pass be more than 90%.The granularity of raw material without it is thin to aforementioned range when, there is γ -2CaOSiO2's The tendency that purity is deteriorated.Specifically, free lime, insoluble residual components become many.
In the present invention, the raw mixture that preferred pair allotment is obtained carries out pelletize.If carrying out pelletize to raw mixture, γ-2CaO·SiO2Reaction of formation become easily to carry out, cost of energy can be cut down, and purity is uprised.
Shape after pelletize is not particularly limited, in rotary kiln is carried out when burning till, it is preferably spherical.In addition, right The size of granules is also not particularly limited, and diameter is preferably 1cm～10cm, more preferably 3cm～7cm.
Pelletize refers to the operation that the raw mixture that allotment is obtained is shaped to ball shape.As its method, can include： Raw mixture and water are put in the rotary drum of collar plate shape to be carried out the method for pelletize, raw mixture is added in a mold and is carried out Press molding, method using so-called comminutor etc..The consumption of the water used during pelletize is preferably by water/raw mixture Mass ratio is calculated as 10～30%, more preferably 15～25%.When the consumption of water is less than 10%, the raw mixture of Jing pelletizes is easy Disintegrate, by dust, sometimes yield is deteriorated raw mixture, and the reaction of burning till when burning till in rotary kiln sometimes is not fully carried out. In addition, when the consumption of water is more than 30%, the washiness in raw mixture after pelletize, still easy disintegrate, sometimes in revolution Reaction of burning till when burning till in kiln is not fully carried out.Further, since more water is included in raw mixture, therefore, in order to incite somebody to action Its evaporation and need it is more burn till energy, thus not only uneconomical, additionally, carrying capacity of environment also becomes big, it is not preferable.
In the present invention, when being burnt till, as the brick of clinkering zone, magnesia spinel class or high-purity alpha-alumina are preferably used Class.It is difficult during using non-magnesia spinel class or high-purity alpha-alumina class, such as silica-alumina brick, magnesium oxide brick Stably to manufacture γ -2CaOSiO2, β -2CaOSiO sometimes2Mix and become obvious.
Herein, as magnesia spinel class brick, high-purity alpha-alumina class brick, the oxidation of JIS R 2302 can be exemplified respectively The refractory brick of the brick of magnesium, the high oxidation aluminum of JIS R 2305.
In the present invention, cooling down operation is carried out after heat treatment, cooling condition is not particularly limited, if do not carry out it is special Quenching operation.Specifically, according to common portland cement clinker cooling condition method, for example return Cooled down by cooler etc. under atmospheric environment after burning till in rotary kiln.
Hereinafter, include embodiment, comparative example to illustrate in greater detail content, but the present invention is not limited to these examples.
Embodiment
[experimental example 1]
Allocate various hydrated lime feeds and siliceous raw material and cause CaO/SiO2Mol ratio is 1.6～2.4.Will with comminutor Allotment raw mixture pelletize glomeration (diameter 4cm).Now, add relative to the water that powder body is 20%.In rotary kiln Heat treatment is carried out to granules.With regard to firing temperature, carry out in the case where the firing temperature of burner is for 1450 DEG C.Need explanation It is that the brick of clinkering zone uses magnesia spinel brick.Burned material to obtaining is analyzed, as a result as shown in table 1.
<Using material>
Hydrated lime feed：Make Acetylenogen. that the Calx for producing by-product after acetylene is reacted with water, by the Calx to by-product The oxide benchmark meter after heat treated is carried out, it is 0.07%, Al that CaO is 73.1%, MgO2O3For 0.55%, Fe2O3For 0.28%th, SiO2For 0.95%, SO3For 1.31%, Na2O is 0.03%, K2It is 23.80% that O is 0.02%, loss on ignition.150μm 99.5%, 100 μm of percent of pass 96.9% of percent of pass.
Siliceous raw material：Silicon stone micropowder, commercially available product, SiO2For 97.05%, Al2O3For 1.89%, Na2O is 0.06%, K2O It is 0.49% for 0.14%, loss on ignition, 7.8 μm of mean diameter, 150 μm of percent of pass, 100%, 100 μm of percent of pass 100%.
Water：Tap water
The brick of clinkering zone：Magnesia spinel brick, content of MgO is 80% and Al2O3Content is 20%.
Rotary kiln：Entrance external diameter 1m, outlet external diameter 1.2m, length 25m
<Assay method>
The identification of compound：Using powder X-ray diffractometry authenticating compound.
The observation of color：White content is judged by visual observation.Observed in the interior of the illumination of 200 luxs, observation is adjusted Whole is 3000 ± 100cm for Blain specific surface2The white content of the powder of/g.It is designated as being designated as during zero, yellow △, brown when white Be designated as during color ×.
[table 1]
S：Strong, is detected with stronger diffraction maximum.
W：Weak, is detected with faint diffraction maximum.
[experimental example 2]
Addition potassium carbonate simultaneously makes total alkali content change like that as shown in table 2 relative to raw mixture, in addition, with reality Testing example 1 is equally carried out.Show the result in table 2.
[table 2]
S：Strong, is detected with stronger diffraction maximum.
W：Weak, is detected with faint diffraction maximum.
[experimental example 3]
In addition to firing temperature is changed as shown in table 3, equally carry out with experimental example 1.Show the result in table 3.
[table 3]
S：Strong, is detected with stronger diffraction maximum.
W：Weak, is detected with faint diffraction maximum.
[experimental example 4]
In addition to the brick of clinkering zone is changed as shown in table 4, carry out in the same manner as experimental example 1.Show the result in Table 4.
<Using material>
High-purity mangesium oxide aluminum brick：Al2O3Content is more than 95%.
Silica-alumina brick：SiO2Content is 30% and Al2O3Content is 70%.
[table 4]
Industrial applicability
γ -2CaOSiO of the invention2Manufacture method, be that carbonating activity is high, whiteness is high, also will not hamper Hinder the condensation hardening of cement, the also high γ -2CaOSiO of cost of energy, yield when burning till can also be cut down2Manufacturer Method, therefore, it is possible to extensively utilize in cement field etc..
In addition, going out to be willing to description, the claim of No. 2012-143769 by Japanese Patent filed in 27 days June in 2012 The full content of book and summary is quoted so far, is incorporated to as the disclosure of the description of the present invention.

Claims (8)

1. a kind of γ -2CaOSiO2Manufacture method, it is characterised in that with firing temperature 1300 DEG C～1600 in rotary kiln DEG C burn till raw mixture, the raw mixture reacts the Calx for producing by-product after acetylene with water compounded with making Acetylenogen. Raw material and siliceous raw material, and carried out adjusting and making CaO/SiO2Mol ratio is more than 1.6 and less than 2.0, total alkali content is 0.10 mass %～1.00 mass %, or make CaO/SiO2Mol ratio is 0.50 matter more than 2.2 and for less than 2.4, total alkali content Amount below %,
Wherein, hydrated lime feed contains the CaO of 71～74 mass %, the loss on ignition of 23～25 mass %, 0.5～1.5 mass % SiO2, 0.2～0.35 mass % Fe2O3, 0.3～0.7 mass % Al2O3, MgO less than 0.2 mass %, any one is equal Less than the Na of 0.1 mass %2O、K2The SO of O and 1.0～1.5 mass %3,
Total alkali content means the Na in terms of quality % contained in raw mixture2O、K2O、Li2The content of O.
2. γ -2CaOSiO according to claim 12Manufacture method, wherein, the brick of the clinkering zone of rotary kiln is magnesia Spinels or high-purity alpha-alumina class.
3. γ -2CaOSiO according to claim 1 and 22Manufacture method, wherein, siliceous raw material be Silicon stone micropowder, silicon The dust of ash, kieselguhr or vitreous silica.
4. γ -2CaOSiO according to claim 1 and 22Manufacture method, wherein, hydrated lime feed and/or siliceous original Material is with 90 mass % above by 150 μm of granularities sieved.
5. γ -2CaOSiO according to claim 1 and 22Manufacture method, wherein, pelletize is carried out to raw mixture, The granules for obtaining are fed to rotary kiln.
6. γ -2CaOSiO according to claim 52Manufacture method, wherein, using pressing the matter of water/raw mixture Amount carries out pelletize than the water for being calculated as 10～30%.
7. γ -2CaOSiO according to claim 1 and 22Manufacture method, wherein, the alkaloid substance in raw mixture For potassium carbonate and/or sodium carbonate.
8. γ -2CaOSiO according to claim 1 and 22Manufacture method, wherein, firing temperature be 1450 DEG C～ 1550℃。
CN201380034489.8A 2012-06-27 2013-06-06 Method for producing gamma-2CaO. SiO2 Active CN104411637B (en)

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CN109467382B (en) * 2018-10-24 2021-05-04 武汉理工大学 Based on gamma-C2S conductive material and preparation method thereof
CN109694224B (en) * 2018-12-19 2021-10-22 武汉理工大学 High-durability concrete product with gradient structure and preparation method thereof
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JP2023061713A (en) * 2021-10-20 2023-05-02 デンカ株式会社 Co2 immobilization material and method for producing co2 immobilization product
WO2023153259A1 (en) * 2022-02-10 2023-08-17 デンカ株式会社 Cement, cement composition, cured cement product, and method for producing cured cement product

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CN103764562A (en) * 2011-08-25 2014-04-30 电气化学工业株式会社 Method for producing gamma-2CaO*SiO2

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